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WO2008095098A2 - Procédé de production de sucre à partir d'une biomasse lignocellulosique utilisant un prétraitement alcalin - Google Patents

Procédé de production de sucre à partir d'une biomasse lignocellulosique utilisant un prétraitement alcalin Download PDF

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Publication number
WO2008095098A2
WO2008095098A2 PCT/US2008/052657 US2008052657W WO2008095098A2 WO 2008095098 A2 WO2008095098 A2 WO 2008095098A2 US 2008052657 W US2008052657 W US 2008052657W WO 2008095098 A2 WO2008095098 A2 WO 2008095098A2
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WO
WIPO (PCT)
Prior art keywords
biomass
alkali
lime
bagasse
conducted
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Application number
PCT/US2008/052657
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English (en)
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WO2008095098A3 (fr
Inventor
Chang-Ho Chung
Donal F. Day
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Board Of Supervisors Of Louisiana State University & Agricultural & Mechanical College
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Application filed by Board Of Supervisors Of Louisiana State University & Agricultural & Mechanical College filed Critical Board Of Supervisors Of Louisiana State University & Agricultural & Mechanical College
Priority to US12/525,354 priority Critical patent/US20100143974A1/en
Publication of WO2008095098A2 publication Critical patent/WO2008095098A2/fr
Publication of WO2008095098A3 publication Critical patent/WO2008095098A3/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P19/00—Preparation of compounds containing saccharide radicals
    • C12P19/02—Monosaccharides
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P7/00—Preparation of oxygen-containing organic compounds
    • C12P7/02—Preparation of oxygen-containing organic compounds containing a hydroxy group
    • C12P7/04—Preparation of oxygen-containing organic compounds containing a hydroxy group acyclic
    • C12P7/06—Ethanol, i.e. non-beverage
    • C12P7/08—Ethanol, i.e. non-beverage produced as by-product or from waste or cellulosic material substrate
    • C12P7/10—Ethanol, i.e. non-beverage produced as by-product or from waste or cellulosic material substrate substrate containing cellulosic material
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P2201/00—Pretreatment of cellulosic or lignocellulosic material for subsequent enzymatic treatment or hydrolysis
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E50/00—Technologies for the production of fuel of non-fossil origin
    • Y02E50/10—Biofuels, e.g. bio-diesel

Definitions

  • T he invention relates to a method for an alkali pretreatment for lignocellulosic biomass to be used in the process of producing simple sugars for fermentation, potentially to ethanol and other useful by-products
  • Additional biomass sources include agricultural residues or wood, including switchgrass waste paper, corn grain, corn cobs, corn husks corn stover, wheat, wheat straw hay, barley, barley straw rice straw, sugar cane bagasse, other grasses, sorghum soy components, trees, branches roots leaves, wood chips , sawdust, shrubs, bush, and combinations thereof
  • Lignin components mainly p-couma ⁇ c acid and ferulic acid, are found in biomass as este ⁇ fied to cell wall polysaccharides (Higuchi, T , Ito, Y , Shimada, M , and Kawamura, I , ( 1967) Phytochemistry 6, 1551 ) Alkali, e g , Ca(OH) 2 or NaOH, reacts with these phenolic acids, even at room temperature, breaking the ester bonds from cell wall polysaccharides and forming salts This addition of alkali (saponification) has been also shown to remove acetyl groups from acetic acid pulp resulting in improvements in cellulose hydrolysis (Pan, Xuejun, Gilkes, Neil and Saddler.
  • This new method included the following steps ( 1 )
  • Raw biomass with sizes up to 10 inches in length for example, sugarcane bagasse
  • the liquid from the above mixture was removed using high pressure, and the liquid stream saved for further product recovery (The liquid stream can be treated with carbonation to capture the calcium as calcium carbonate or the leftover liquid can be used as a source for the chemical 4-ethylphenol)
  • the pH of the solids was adjusted using acid to a pH appropriate for cellulase hydrolysis
  • cellulase was added to hydrolyze the cellulose to simple sugars
  • This method does not have a particle reduction step, as long as the starting material is less than or equal to about 10 inches in length, e g , bagasse from the mill
  • the pressing step removes both lignin and the alkali which prevents inhibition of the enzymes used in hydrolysis
  • only 0 2 g lime/ g of dry solid bagasse was used The method described above was capable of being enz ⁇ me solub
  • FIG. 1 illustrates the cellulose hydrolysis over time as a percent of the theoretical cellulose hydrolysis using a 1 % (w/v) glucan loading for AVICEL® (a synthetic biopolymer) and for lime-treated bagasse.
  • FIG. 2 illustrates the cellulose hydrolysis over time as a percent of the theoretical cellulose hydrolysis using a 10% (w/v) solids (which equates to a 4% (w/v) glucan) loading for AVICEL® (a synthetic biopolymer), for lime-treated bagasse and for bagasse without lime-treatment (Control).
  • AVICEL® a synthetic biopolymer
  • FIG. 3 illustrates the effect of various levels of glucan loading with AVICEL®
  • Fig. 4 illustrates the hydrolysis and fermentation profile for the concentration of glucose, xylose and ethanol in a pilot scale test using 17.6% (w/w) dry solid loading of bagasse after lime pretreatment.
  • Fig. 5 illustrates the effect of various concentrations of lime (0, 0.02, 0.05, 0.1 and 0.2 g lime/ g dry solid bagasse) used for 10% solid loading (or 4% glucan) on the yield of fermentable sugar measured as the percent of the theoretical cellulose hydrolysis at two different time frames, 24 hr and 90 hr.
  • the liquid is removed just after the heating treatment, so that most of the lime was recovered in the liquid portion
  • the fibrous solid material that remained was then used for hydrolysis by cellulase enzymes
  • this lime pretreatment and pressing step the structure of the lignocellulosic material was modified such that it was rapidly solubilized by cellulase, even at high solids loading ( 10-30%) without an inhibitory effect on the cellulase activity
  • This process is unique among proposed pretreatments for biomass, including other proposed lime treatments, in the ability to remove the lime residue and the solubhzation of lignocellulose at greater than 5% solids loading
  • this process did not produce enzyme inhibitors
  • the pressing step increases the lignin in solution and increases the removal of alkali so that less inhibitors are present for enzyme hydrolysis
  • This treatment offers numerous advantages over what is currently proposed for conversion of lignocellulosic materials to ethanol, especially by allowing hydrolysis at high solids loading, which is a
  • This method should work on all lignocellulosic material, including switchgrass, waste paper, corn grain, corn cobs, corn husks, corn stover, wheat, wheat straw, hay, barley, barley straw, rice straw, sugar cane bagasse, other grasses, sorghum, soy components, trees, branches roots, leaves, wood chips , sawdust, shrubs, bush, and combinations thereof
  • the starting lignocellulosic material should be of a size less than or equal to about 25 cm length, more preferably less than about 15 cm in length, and most preferably less than about 10 cm in length Sugarcase bagasse can be used as is Other materials may have to be chopped to meet this size limitation However, this method does not require the grinding of any sample into particle sizes less than a centimeter
  • alkali material could be used for the pretreatment as long as the pH is increased above 1 1 5 to remove the hgnin
  • alkali useful for the disclosed method include any mineral alkali, any alkali metal hydroxide, alkaline earth metal hydroxide or alkaline earth metal oxide, including sodium hydroxide, potassium hydroxide calcium oxide, calcium hydroxide, lithium hydroxide, rubidium hydroxide, etc
  • the preferred alkali for bioethanol production is the most economical one, which currently is lime (calcium oxide) jOO 18]
  • An effective use of lime has many benefits ( 1 ) Alkaline preireaimenis, iike lime, degrade lignin and leave the cellulose and hemiceliulose intact; (2) cellulase inhibitors are not formed from the lignin portion as occurs with acid pretreatments; (3) lime is the least expensive base that could be used; (4) lime is more environmentally friendly than other potential bases; (5) lime is relatively easy to recover as calcium salt; and (6) use of lime in industry is
  • the temperature of the alkali pretreatinent step depends on the concentration of the alkali and the biomass, and depends on the time for the process.
  • the range of temperature is from about 50 0 C to about 150 0 C, with a preferred range of about 8O 0 C to about 140 0 C.
  • the time for the alkali pretreatment is from about 20 min to about 10 hr, with the preferred range of about 20 min to 6 hr.
  • the temperature and pH must be adjusted to levels compatible with the enzymes to be added for hydrolysis.
  • the potential range in temperature for enzymatic hydrolysis is from about 20 0 C to about 70 0 C, with a preferred range of about 28°C to about 55 0 C.
  • the pH range can be from about 4 to about 7, with a preferred range of about 4.5 to about 5.5.
  • the pH can be adjusted after the alkali pretreatment with an acid, for example, with sulfuric acid, hydrochloric acid, or hydrofluoric acid. The only limitation is whether the acid would form salts that would inhibit the enzymes. For bioethanol production, sulfuric acid is currently preferred as being the most cost-effective.
  • any known fermentation organism can be used, including yeast (Saccharomyces cerevisiae), and other microorganisms (recombinant Escherichia colt. Zymomonas mobihs, Bacillus stearothermophilus, and Pichia stipitis), either naturally -occurring or genetically modified.
  • yeast Sacharomyces cerevisiae
  • microorganisms recombinant Escherichia colt. Zymomonas mobihs, Bacillus stearothermophilus, and Pichia stipitis
  • an inexpensive sugar source may be added to the fermentation step, e.g., molasses.
  • Enzy me lndrolysis The lime-treated bagasse was subjected to enzyme hydrolysis, w ithout sterilization in large flasks The pH was adjusted with sulfuric acid to an enzyme optimum pH 4.8-5 2. The ⁇ r ⁇ change by residual iime discharge from the treated bagasse was monitored with an extra sample and additional sulfuric acid was added if necessary to maintain the pH range close to optimum for enzymatic activity.
  • Enzymatic hydrolysis of the cellulose residue was conducted using commercially available enzymes, Spezyme CP (Genencor International Co., Cedar Rapids, Iowa) and Novol 88 (Novozyme; Salem, Virginia). The enzyme activity was measured as Filter Paper Units/ gram solid (FPU/g solid) according to NREL procedure.
  • the cellobiase activity was given by the manufacturer. Enzyme saccharifications were measured by NREL methods (NREL at the website, accessed November 2006. The concentrations of the enzymes used were cellulase (60 FPU/g of glucan) and celiobiase (64 CBU/g of glucan). The amount of hydrolysis was followed over time. In the event of greater than 10% (w/w) solid loading, the flasks were agitated at 180 rpm during enzyme hydrolysis and at 100 rpm for fermentation because of the high viscosity of the slurry. AVICEL® (Ph- 102; FMC Biopolymer, Philadelphia, Pennsylvania) was used as a control. The following formula was used to calculate percent of theoretical of cellulose hydrolysis (NREL LAP-008; http //www eere energy gov/b ⁇ omass/analyt ⁇ cal_procedures html accessed Nov. 2006 )
  • glucose represents the residual glucose concentration
  • (EtOH) f " represents the ethanol concentration (g/L) at the end of the fermentation minus any ethanol produced from the enzyme and medium
  • (Biomass/ ' represents the dry biomass (in most experiments, bagasse) concentration (g/L) at the beginning of the fermentation
  • "f represents the cellulose fraction in dry biomass(g/g) as calculated from the composition analysis
  • 0 51 " is the conversion factor for glucose to ethanol based on stoichiometric biochemistry of yeast
  • 1 1 1 1 is the conversion factor for cellulose to equivalent glucose
  • Pilot Bioethanol Production Pilot-scale bioethanol production was demonstrated using a 120 L sugar crystallizer as a reactor vessel, equipped with the ability to mix and to control the temperature
  • the reactor had a horizontal rotary shaft mounted with paddles for mixing The mixing speed was set at 8 rpm per minute
  • sulfuric acid was added
  • Tap w ater was added to get 18 % (w/w) dry solid loading
  • the initial enzyme loading was 60 FPU/g glucan (Spe7yme CP) and 64 CBU/g glucan (Novo l 88), and the temperature raised to 50 0 C
  • a pH control problem was encountered in the early stages of enzyme hydrolysis that caused the enzymes to become inactivated The problem was confirmed by a separate enzyme activity test of the collected samples (data not ⁇ own)
  • Table 1 Composition analysis of bagasse before and after lime treatment (% dry wt)
  • F ig 2 illustrates the percent theoretical of cellulose hvdroK sis using 10% solids, or a 4° o glucan loading (w/v)
  • Fig 2 at a level of 4% glucan (equivalent to 10 0% solid loading containing 40% gluca ⁇ ), th e 'reated bagasse h> dro!> ?ed better than AVICFL&
  • AVICEL® End ⁇ i ⁇ ducib such as glucose and eeiiobiose are known to oe inhibitors of enzyme hydrolysis in high solid loading
  • yeast was added to relieve the end product inhibition, the % of theoretical ethanol > ields from cellulose still decreased with an increase in solid loadings This decrease in conversion may be related to other factors, such as differences in diffusion rate water availability , osmotic pressure and/or sugars from hemicellulose in high solid loading
  • Table 3 Results from SHF of pilot scale trial on bagasse.

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  • Organic Chemistry (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Zoology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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  • General Chemical & Material Sciences (AREA)
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Abstract

L'invention concerne un nouveau procédé de traitement d'une biomasse avec un alcali, par exemple de la chaux. La chaux et la lignine sont suffisamment éliminées de la biomasse traitée par extraction par pression avec un dispositif haute pression afin d'éliminer les alcalis et autres inhibiteurs potentiels des enzymes cellulase ajoutées pour la saccharification. Le matériau fibreux résultant est rapidement solubilisé par des cellulases, même à des charges en solides comprises entre 10 et 30 % (m/m) sans effets d'inhibition sur l'activité cellulase. Le prétraitement par la chaux élimine la lignine de manière efficace et laisse la cellulose et l'hémicellulose pratiquement intactes. Le procédé permet d'obtenir une biomasse ayant une structure capable d'être solubilisée par des enzymes et fermentée facilement à une charge en solides de 10 à 30 % pour la fabrication d'éthanol.
PCT/US2008/052657 2007-02-01 2008-01-31 Procédé de production de sucre à partir d'une biomasse lignocellulosique utilisant un prétraitement alcalin WO2008095098A2 (fr)

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US12/525,354 US20100143974A1 (en) 2007-02-01 2008-01-31 Process for Sugar Production from Lignocellulosic Biomass Using Alkali Pretreatment

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US88768407P 2007-02-01 2007-02-01
US60/887,684 2007-02-01

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Cited By (25)

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WO2009135898A3 (fr) * 2008-05-07 2010-01-21 Novozymes A/S Fermentation d'une matière contenant de la lignocellulose
WO2010076552A1 (fr) 2008-12-29 2010-07-08 Petróleo Brasileiro S A -Petrobras Procédé de production d'une préparation enzymatique pour l'hydrolyse de cellulose à partir de résidus lignocellulosiques, et son application dans la production d'éthanol
WO2010059891A3 (fr) * 2008-11-20 2010-10-28 E. I. Du Pont De Nemours And Company Procédé de production d'une solution de sucre concentrée par saccharification enzymatique d'une biomasse enrichie en polysaccharide
WO2010124944A1 (fr) 2009-04-28 2010-11-04 Heli Inovatio Handelsbolag Procédé pour l'hydrolyse de la cellulose
WO2010113129A3 (fr) * 2009-03-31 2010-12-29 Chemtex Italia S.R.L. Procédé de prétraitement de biomasse perfectionné
WO2010060052A3 (fr) * 2008-11-21 2011-01-06 North Carolina State University Production d'éthanol à partir de biomasse lignocellulosique utilisant un prétraitement à la liqueur verte
US7943363B2 (en) 2008-07-28 2011-05-17 University Of Massachusetts Methods and compositions for improving the production of products in microorganisms
US20110143411A1 (en) * 2009-11-13 2011-06-16 Fpinnovations Biomass fractionation process for bioproducts
FR2963009A1 (fr) * 2010-07-23 2012-01-27 IFP Energies Nouvelles Procede de production de sucres a partir de biomasse lignocellulosique pretraitee avec des sels inorganiques hydrates
WO2012057684A1 (fr) 2010-10-27 2012-05-03 Heli Inovatio Handelsbolag Procédé de dérivation de la cellulose
CN101619332B (zh) * 2009-08-13 2012-05-23 安徽丰原发酵技术工程研究有限公司 一种甘蔗渣高效糖化的方法
CN101613727B (zh) * 2009-07-21 2012-06-13 安徽丰原发酵技术工程研究有限公司 一种生物质制糖方法
WO2012047832A3 (fr) * 2010-10-07 2012-08-23 Shell Oil Company Procédé de production d'alcools à partir de biomasse
EP2496701A2 (fr) * 2009-11-02 2012-09-12 Hercules Incorporated Procédé de traitement de biomasse pour augmenter l'accessibilité des polysaccharides qui y sont contenus à l'hydrolyse et à la fermentation ultérieure, et polysaccharides à accessibilité augmentée
CN102703520A (zh) * 2012-05-22 2012-10-03 中国科学院广州能源研究所 一种蔗渣水解液和糖蜜混合发酵生产乙醇的方法
US8304535B2 (en) 2008-11-20 2012-11-06 E I Du Pont De Nemours And Company Sugar production by decrystallization and hydrolysis of polysaccharide enriched biomass
US8372609B2 (en) 2008-11-20 2013-02-12 E I Du Pont De Nemours And Company Process for producing a sugar solution by combined chemical and enzymatic saccharification of polysaccharide enriched biomass
WO2013131162A1 (fr) * 2012-03-08 2013-09-12 Companhia Paulista De Força E Luz - Cpfl Procédé de production de bioéthanol à partir du pseudo-tronc du bananier par hydrolyse enzymatique, et utilisation de celui-ci
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CN103957726A (zh) * 2011-04-13 2014-07-30 Ensus有限公司 用于动物饲料生产的水解和发酵方法
EP2732055A4 (fr) * 2011-07-15 2015-03-11 Greenfield Specialty Alcohols Inc Conditionnement de biomasse pour libération de sucre en c5/c6 améliorée avant fermentation
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WO2009135898A3 (fr) * 2008-05-07 2010-01-21 Novozymes A/S Fermentation d'une matière contenant de la lignocellulose
US8435771B2 (en) 2008-05-07 2013-05-07 Novozymes A/S Fermentation of a lignocellulose-containing material
US7943363B2 (en) 2008-07-28 2011-05-17 University Of Massachusetts Methods and compositions for improving the production of products in microorganisms
US8304535B2 (en) 2008-11-20 2012-11-06 E I Du Pont De Nemours And Company Sugar production by decrystallization and hydrolysis of polysaccharide enriched biomass
WO2010059891A3 (fr) * 2008-11-20 2010-10-28 E. I. Du Pont De Nemours And Company Procédé de production d'une solution de sucre concentrée par saccharification enzymatique d'une biomasse enrichie en polysaccharide
US8524474B2 (en) 2008-11-20 2013-09-03 E I Du Pont De Nemours And Company Process for producing a concentrated sugar solution by enzymatic saccharification of polysaccharide enriched biomass
US8372609B2 (en) 2008-11-20 2013-02-12 E I Du Pont De Nemours And Company Process for producing a sugar solution by combined chemical and enzymatic saccharification of polysaccharide enriched biomass
WO2010060052A3 (fr) * 2008-11-21 2011-01-06 North Carolina State University Production d'éthanol à partir de biomasse lignocellulosique utilisant un prétraitement à la liqueur verte
US20110314726A1 (en) * 2008-11-21 2011-12-29 Hasan Jameel Production of ethanol from lignocellulosic biomass using green liquor pretreatment
WO2010076552A1 (fr) 2008-12-29 2010-07-08 Petróleo Brasileiro S A -Petrobras Procédé de production d'une préparation enzymatique pour l'hydrolyse de cellulose à partir de résidus lignocellulosiques, et son application dans la production d'éthanol
WO2010113129A3 (fr) * 2009-03-31 2010-12-29 Chemtex Italia S.R.L. Procédé de prétraitement de biomasse perfectionné
US9234224B2 (en) 2009-03-31 2016-01-12 Beta Renewables, S.p.A. Biomass pretreatment process
US8758517B2 (en) 2009-04-28 2014-06-24 Re:Newcell Lux S.A.R.L Process for the hydrolysis of cellulose
WO2010124944A1 (fr) 2009-04-28 2010-11-04 Heli Inovatio Handelsbolag Procédé pour l'hydrolyse de la cellulose
CN101613727B (zh) * 2009-07-21 2012-06-13 安徽丰原发酵技术工程研究有限公司 一种生物质制糖方法
CN101619332B (zh) * 2009-08-13 2012-05-23 安徽丰原发酵技术工程研究有限公司 一种甘蔗渣高效糖化的方法
EP2496701A2 (fr) * 2009-11-02 2012-09-12 Hercules Incorporated Procédé de traitement de biomasse pour augmenter l'accessibilité des polysaccharides qui y sont contenus à l'hydrolyse et à la fermentation ultérieure, et polysaccharides à accessibilité augmentée
US9580454B2 (en) * 2009-11-13 2017-02-28 Fpinnovations Biomass fractionation process for bioproducts
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